CN109485669B - Production line for producing trimethylchlorosilane by tower stacking method and production method thereof - Google Patents
Production line for producing trimethylchlorosilane by tower stacking method and production method thereof Download PDFInfo
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- CN109485669B CN109485669B CN201811402192.3A CN201811402192A CN109485669B CN 109485669 B CN109485669 B CN 109485669B CN 201811402192 A CN201811402192 A CN 201811402192A CN 109485669 B CN109485669 B CN 109485669B
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- IJOOHPMOJXWVHK-UHFFFAOYSA-N chlorotrimethylsilane Chemical compound C[Si](C)(C)Cl IJOOHPMOJXWVHK-UHFFFAOYSA-N 0.000 title claims abstract description 78
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 66
- 239000005051 trimethylchlorosilane Substances 0.000 title claims abstract description 39
- 238000000034 method Methods 0.000 title claims abstract description 37
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 127
- 239000007789 gas Substances 0.000 claims abstract description 115
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 claims abstract description 107
- 229910000041 hydrogen chloride Inorganic materials 0.000 claims abstract description 107
- 238000006243 chemical reaction Methods 0.000 claims abstract description 99
- UQEAIHBTYFGYIE-UHFFFAOYSA-N hexamethyldisiloxane Chemical compound C[Si](C)(C)O[Si](C)(C)C UQEAIHBTYFGYIE-UHFFFAOYSA-N 0.000 claims abstract description 67
- 238000010438 heat treatment Methods 0.000 claims abstract description 64
- 238000012856 packing Methods 0.000 claims abstract description 20
- 239000007921 spray Substances 0.000 claims description 39
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 32
- 230000000903 blocking effect Effects 0.000 claims description 24
- 238000005507 spraying Methods 0.000 claims description 24
- 239000007788 liquid Substances 0.000 claims description 21
- 239000002994 raw material Substances 0.000 claims description 18
- 239000000498 cooling water Substances 0.000 claims description 15
- 238000001816 cooling Methods 0.000 claims description 14
- 230000000694 effects Effects 0.000 claims description 11
- 239000000945 filler Substances 0.000 claims description 9
- 238000003860 storage Methods 0.000 claims description 9
- 239000000376 reactant Substances 0.000 claims description 7
- 238000004064 recycling Methods 0.000 claims description 7
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 claims description 4
- 238000009833 condensation Methods 0.000 claims description 4
- 230000005494 condensation Effects 0.000 claims description 4
- 229910052731 fluorine Inorganic materials 0.000 claims description 4
- 239000011737 fluorine Substances 0.000 claims description 4
- 238000005086 pumping Methods 0.000 claims description 4
- 238000012546 transfer Methods 0.000 claims description 4
- 238000007599 discharging Methods 0.000 claims description 3
- 239000011521 glass Substances 0.000 claims description 3
- 238000010992 reflux Methods 0.000 claims description 3
- 238000003303 reheating Methods 0.000 claims description 3
- 230000003014 reinforcing effect Effects 0.000 claims description 3
- 239000005046 Chlorosilane Substances 0.000 claims description 2
- KOPOQZFJUQMUML-UHFFFAOYSA-N chlorosilane Chemical compound Cl[SiH3] KOPOQZFJUQMUML-UHFFFAOYSA-N 0.000 claims description 2
- 230000036961 partial effect Effects 0.000 claims description 2
- 230000008569 process Effects 0.000 claims description 2
- 230000001737 promoting effect Effects 0.000 abstract description 6
- 238000011084 recovery Methods 0.000 abstract description 4
- 230000002829 reductive effect Effects 0.000 description 13
- 230000014759 maintenance of location Effects 0.000 description 10
- 239000000047 product Substances 0.000 description 8
- 239000003814 drug Substances 0.000 description 4
- 229940079593 drug Drugs 0.000 description 4
- 125000004122 cyclic group Chemical group 0.000 description 3
- 238000005265 energy consumption Methods 0.000 description 3
- 238000009776 industrial production Methods 0.000 description 3
- 238000001556 precipitation Methods 0.000 description 3
- 230000000717 retained effect Effects 0.000 description 3
- 239000002699 waste material Substances 0.000 description 3
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 239000006227 byproduct Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000000630 rising effect Effects 0.000 description 2
- 239000002912 waste gas Substances 0.000 description 2
- 230000009471 action Effects 0.000 description 1
- 235000019270 ammonium chloride Nutrition 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 239000002440 industrial waste Substances 0.000 description 1
- 230000000670 limiting effect Effects 0.000 description 1
- 238000005007 materials handling Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002304 perfume Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 238000006884 silylation reaction Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 235000011149 sulphuric acid Nutrition 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F7/00—Compounds containing elements of Groups 4 or 14 of the Periodic Table
- C07F7/02—Silicon compounds
- C07F7/08—Compounds having one or more C—Si linkages
- C07F7/12—Organo silicon halides
- C07F7/121—Preparation or treatment not provided for in C07F7/14, C07F7/16 or C07F7/20
- C07F7/123—Preparation or treatment not provided for in C07F7/14, C07F7/16 or C07F7/20 by reactions involving the formation of Si-halogen linkages
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Silicon Compounds (AREA)
Abstract
The invention relates to a production line for producing trimethylchlorosilane by a tower-stacking method, which comprises a packing rectifying tower, a plate type reaction tower and a heating kettle which are sequentially arranged from top to bottom, wherein the bottom of the packing rectifying tower is communicated with the top of the plate type reaction tower, the top of the heating kettle is connected with the side wall of the lower part of the plate type reaction tower through a communicating pipe, a hexamethyldisiloxane inlet pipe is arranged on the outer wall of the upper part of the plate type reaction tower, a hydrogen chloride inlet gas pipe for introducing dry hydrogen chloride gas is connected onto the side wall of the heating kettle, the top of the packing rectifying tower is connected with a condenser through an air outlet pipe, the bottom of the condenser is connected with the side wall of the upper part, the invention provides a production line and a production method for producing trimethylchlorosilane by a tower stacking method, which have the advantages of low production cost, simple structure, high production efficiency, good reaction promoting effect, high recovery and utilization rate and long service life.
Description
Technical Field
The invention relates to a production line for producing trimethylchlorosilane by a tower stacking method and a production method thereof.
Background
The trimethylchlorosilane is an important protective silylation reagent and is widely applied to the synthesis of perfumes and organic medicines, with the development of cephalo-type medicines in recent years, the application of the cephalo-type medicines is more and more extensive, the demand is more and more, a large amount of cephalo-type medicines are imported every year to meet the demand, the trimethylchlorosilane is mainly obtained by converting hexamethyldisiloxane, and the production method mainly comprises the following steps: 1. the SOCL2 method, in which hexamethyldisiloxane is reacted with SOCL2, produces SO2 as a by-product, and the amount of SOCL2 is large, which is not convenient for industrial use; 2. the method of concentrated H2SO4+ ammonium chloride, the hydrogen chloride generated by the reaction reacts with hexamethyldisiloxane, the generated water is absorbed by concentrated sulfuric acid, the three wastes are large, the production cost is high, and the method is difficult to be applied to industrial production; 3. according to the PCL5 method, a by-product of the reaction is POCL3, which can better meet the industrial production, but the process has high requirement on the purity of hexamethyldisiloxane (the content is more than 98 percent); 4. the ALCL3 method has the advantages of low yield (77%), low purity, large quantity of three wastes and difficult adoption of industrial production; 5. the hydrogen chloride method has great difficulty in application to production, or requires a reaction at a temperature below-20 ℃ or a reaction at a pressure of more than 1.47Mpa, the production equipment has high requirements, the existing production method for producing trimethylchlorosilane has high production cost, large occupied area of the production equipment, high investment and high requirements of the reaction on production, the precision of conveying equipment among all connecting parts has high requirements, meanwhile, the service life of each conveying equipment is greatly reduced due to the corrosivity of products, meanwhile, the production efficiency is low, substances after the reaction cannot be fully recycled, the resource consumption is high, the reaction efficiency of a reaction tower for the reaction is low, the requirement of increasing the yield cannot be met, and the reaction promoting effect is limited.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide the production line and the production method for producing the trimethylchlorosilane by the tower stacking method, which have the advantages of low production cost, simple structure, high production efficiency, good reaction promoting effect, high recycling rate and long service life.
The technical scheme of the invention is realized as follows: a production line for producing trimethylchlorosilane by a tower stacking method is characterized in that: comprises a packing rectifying tower (1), a plate-type reaction tower (2) and a heating kettle (3) which are sequentially arranged from top to bottom, wherein the bottom of the packing rectifying tower (1) is communicated with the top of the plate-type reaction tower (2), the top of the heating kettle (3) is connected with the lower side wall of the plate-type reaction tower (2) through a communicating pipe (4), a hexamethyldisiloxane inlet pipe (5) is arranged on the outer wall of the upper part of the plate-type reaction tower (2), a hydrogen chloride inlet gas pipe (6) for leading in dry hydrogen chloride gas is connected onto the side wall of the heating kettle (3), a condenser (8) is connected onto the top of the packing rectifying tower (1) through an outlet pipe (7), the bottom of the condenser (8) is connected with the upper side wall of the packing rectifying tower (1) through a return pipe (9), and a chlorosilane discharging pipe (10) for leading out trimethyl is arranged on, plate-type reaction tower (2) bottom is kept away from into one side lateral wall of hydrogen chloride gas pipe (6) through outlet pipe (21) and heating cauldron (3) and is connected, heating cauldron (3) bottom is provided with drain pipe (22) that are used for deriving the dilute hydrochloric acid.
Preferentially, the method comprises the following steps: condenser (8) outside cover is equipped with cooler bin (11), be connected with circulating water inlet tube (12) that are used for letting in the cooling water on the lateral wall of cooler bin (11) one side, be connected with circulating water wet return (13) that are used for deriving the cooling water after the heat transfer on the lateral wall of one side that circulating water inlet tube (12) was kept away from in cooler bin (11).
Preferentially, the method comprises the following steps: condenser (8) top is connected with muffler (14) that are used for deriving surplus hydrogen chloride gas, muffler (14) are kept away from behind condenser (8) the one end run through cooling tank (11) lateral wall with advance hydrogen chloride gas pipe (6) intercommunication, be provided with fan (15) on muffler (13).
Preferentially, the method comprises the following steps: and a hydrogen chloride vent valve (16) is arranged on the hydrogen chloride inlet gas pipe (6).
Preferentially, the method comprises the following steps: plate-type reaction tower (2) is including being vertical cylindric tower body (100), the one end and tower body (100) lower part lateral wall that heating cauldron (3) were kept away from to communicating pipe (4) are connected, tower body (100) are inside and lie in communicating pipe (4) top and be provided with first spray assembly and second spray assembly respectively, first spray assembly includes from last first ring pipe (111) and first filter plate (112) down set gradually, be provided with a plurality of first shower (113) along circumference equidistance interval each other on first ring pipe (111) lateral wall, the second spray assembly includes from last second ring pipe (121) and the second filter plate (122) that down set gradually, be provided with a plurality of second shower (123) along circumference equidistance interval each other on second ring pipe (121) lateral wall, first filter plate (112) and second filter plate (122) upper surface all evenly pile up and are provided with a plurality of being used for hindering and stay hexamethyldisiloxane cooperation hydrogen chloride gas The body carries out the trapping ring subassembly that reacts, hexamethyldisiloxane advances pipe (5) one end and is connected with first ring pipe (111) and second ring pipe (121) respectively, hexamethyldisiloxane advances one end that pipe (5) kept away from tower body (100) and is connected with storage hexamethyldisiloxane case (104), hexamethyldisiloxane advances to be provided with on pipe (5) and sprays pump (105), the tower body bottom is provided with cistern (102), cistern (102) are connected with heating cauldron (3) lateral wall through outlet pipe (21), gas outlet (103) and filler rectifying column (1) bottom intercommunication are passed through to tower body (100) top.
Preferentially, the method comprises the following steps: the detaining ring assembly comprises a plurality of connecting rings (131) which are distributed on the same central shaft at equal intervals along the longitudinal direction, a central column (132) is arranged on the central shaft of the connecting rings (131), a plurality of detaining plates (133) are arranged on the side wall of the central column (132) along the circumferential direction and between the adjacent connecting rings (131), and the adjacent connecting rings (131) are fixedly connected with each other through the plurality of detaining plates (133).
Preferentially, the method comprises the following steps: the blocking plates (133) are arranged at intervals along the circumferential direction of the central column (132) at equal intervals, and a reinforcing blocking plate (134) is arranged between every two adjacent blocking plates (133).
Preferentially, the method comprises the following steps: one end of the first spray pipes (113) far away from the first annular pipe (111) is deviated towards the longitudinal central axis of the tower body (100), and one end of the second spray pipes (123) far away from the second annular pipe (121) is deviated towards the longitudinal central axis of the tower body (100).
Preferentially, the method comprises the following steps: the connecting ring (131), the central column (132), the blocking plate (133) and the reinforced blocking plate (134) are all made of glass lining and fluorine-containing plastic.
The invention also discloses a production method of the production line for producing trimethylchlorosilane by the tower stacking method, which has low energy consumption and high cyclic utilization rate, and comprises the following steps:
1) and raw material feeding: the spraying pump (105) runs normally, hexamethyldisiloxane in the hexamethyldisiloxane storage box (104) is pumped and continuously introduced into a first annular pipe (111) and a second annular pipe (121) in the plate-type reaction tower (2) through the hexamethyldisiloxane inlet pipe (5), and the hexamethyldisiloxane is sprayed downwards from a plurality of first spraying pipes (113) arranged on the side wall of the first annular pipe (111) and a plurality of second spraying pipes (123) arranged on the side wall of the second annular pipe (121), and the flow rate of the hexamethyldisiloxane is controlled by the spraying pump (105) to be 200 kg/h;
2) and introducing reactants: opening a hydrogen chloride vent valve (16), introducing dry hydrogen chloride gas into a heating kettle (3) from a hydrogen chloride gas inlet pipe (6), operating the heating kettle (3) and heating the dry hydrogen chloride gas, introducing the heated hydrogen chloride gas into a plate-type reaction tower (2) from a communicating pipe (4) arranged at the top of the heating kettle (3), and controlling the flow of the dry hydrogen chloride gas to be 110 kg/h;
3) and reaction rectification: hexamethyldisiloxane is respectively and uniformly sprayed to a blocking ring assembly on the upper surfaces of a first filter plate 112 and a second filter plate 122 and is fully blocked on a plurality of connecting rings (131), a central column (132) and a plurality of blocking plates (133), hydrogen chloride gas heated and dried rises from the bottom of a plate-type reaction tower (2) and reacts with the hexamethyldisiloxane, the gas rises from a gas outlet (103) at the top of the plate-type reaction tower (2) after reaction and enters a packing rectifying tower (1) for rectification, the reacted water is mixed with hydrogen chloride to form dilute hydrochloric acid liquid, the dilute hydrochloric acid liquid falls into a reservoir (102), the dilute hydrochloric acid liquid flows back into a heating kettle (3) from a water outlet pipe (21), and the dilute hydrochloric acid liquid is led out through a liquid outlet pipe (22) arranged at the bottom of the heating kettle (3);
4) condensing and refluxing: the condenser (8) works, cooling water is continuously introduced into the condenser (8) and enters the cooling box (11) from the circulating water inlet pipe (12) to be matched with the cooler (8) for cooling, the cooling water after heat exchange is led out from the circulating water return pipe (13), gaseous hydrogen chloride and trimethylchlorosilane rise and enter the condenser (8) from the gas outlet pipe (7), a trimethylchlorosilane finished product is led out from the discharge pipe (10) on the side wall of the condenser (8) under the condensation effect, and partial liquid flows back to the filler rectifying tower (1) from the bottom of the condenser (8) through the return pipe (9) to be rectified again to improve the purity;
5) and (3) circulating reaction: and (3) opening the fan (15), keeping the micro negative pressure in the air return pipe (14) between 0 and-0.01 Mpa, pumping the residual hydrogen chloride gas in the condenser (8) from the air return pipe (14) back to the hydrogen chloride gas inlet pipe (6), and returning the residual hydrogen chloride gas to the heating kettle (3) to be mixed with the dry hydrogen chloride gas for reheating and recycling.
By adopting the technical scheme, the packed rectifying tower (1), the plate-type reaction tower (2) and the heating kettle (3) for reaction are sequentially arranged from top to bottom, so that on one hand, various conveying devices for conveying reactants and products are reduced, the production line is simplified, the production cost is reduced, the floor area of the production device is reduced, the structure is relatively simple, on the other hand, after the dry hydrogen chloride gas enters the heating kettle (3) for heating, the dry hydrogen chloride gas quickly rises into the plate-type reaction tower (2) to be in full contact reaction with hexamethyldisiloxane in the plate-type reaction tower (2), the reaction efficiency is improved, meanwhile, the hexamethyldisiloxane is fully retained by the retaining ring assembly arranged in the plate-type reaction tower (2), and the spraying effect of the first spraying assembly and the second spraying assembly is matched, and the hydrogen chloride gas after the drying and heating which rises from bottom to top is subjected to uniform contact reaction, the overall efficiency of the reaction is improved, the residual hydrogen chloride gas in the condenser (8) after the reaction is finished is pumped back into the hydrogen chloride gas inlet pipe (6) from the gas return pipe (14) and flows back into the heating kettle (3) to be mixed with the dried hydrogen chloride gas for recycling after being reheated, the overall resource recovery utilization rate is improved, the overall production cost is further reduced, the emission of waste gas is reduced, the precipitation efficiency of the product trimethylchlorosilane is further improved by matching the cooling box (11) with the condenser (8), the overall production speed is improved, meanwhile, the water obtained by the reaction in the plate-type reaction tower (2) is mixed with the hydrogen chloride gas to generate dilute hydrochloric acid, the dilute hydrochloric acid is uniformly led out through a liquid outlet pipe (22) arranged at the bottom of the heating kettle (3), and the treatment of waste water is facilitated, the invention provides a production line and a production method for producing trimethylchlorosilane by a tower stacking method, which have the advantages of low production cost, simple structure, high production efficiency, good reaction promoting effect, high recovery and utilization rate and long service life.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to these drawings without creative efforts.
FIG. 1 is a schematic structural diagram of an embodiment of the present invention.
FIG. 2 is a schematic diagram of a plate-type reaction tower according to an embodiment of the present invention.
Fig. 3 is a schematic front view of a detainer ring assembly in accordance with an embodiment of the present invention.
Figure 4 is a schematic top view of a blocker ring assembly according to one embodiment of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
As shown in fig. 1-4, the invention discloses a production line for producing trimethylchlorosilane by a tower-stacking method, in the specific embodiment of the invention, the production line comprises a filler rectifying tower 1, a plate-type reaction tower 2 and a heating kettle 3 which are sequentially arranged from top to bottom, the bottom of the filler rectifying tower 1 is communicated with the top of the plate-type reaction tower 2, the top of the heating kettle 3 is connected with the side wall of the lower part of the plate-type reaction tower 2 through a communicating pipe 4, the outer wall of the upper part of the plate-type reaction tower 2 is provided with a hexamethyldisiloxane inlet pipe 5, the side wall of the heating kettle 3 is connected with a hydrogen chloride inlet gas pipe 6 for introducing dry hydrogen chloride gas, the top of the filler rectifying tower 1 is connected with a condenser 8 through an air outlet pipe 7, the bottom of the condenser 8 is connected with the side wall of the upper part of the filler rectifying tower 1 through a return, the bottom of the plate-type reaction tower 2 is connected with one side wall of the heating kettle 3 far away from the hydrogen chloride gas inlet pipe 6 through a water outlet pipe 21, and the bottom of the heating kettle 3 is provided with a liquid outlet pipe 22 for leading out dilute hydrochloric acid.
By adopting the technical scheme, the packing rectifying tower 1, the plate-type reaction tower 2 and the heating kettle 3 are sequentially arranged from top to bottom, the bottom of the packing rectifying tower 1 is communicated with the top of the plate-type reaction tower 2, the side wall of the heating kettle 3 is connected with a hydrogen chloride gas inlet pipe 6 for introducing dry hydrogen chloride gas, the dry hydrogen chloride gas enters the heating kettle 3 from the hydrogen chloride gas inlet pipe 6 to be heated, after the heating is finished, the hydrogen chloride gas enters the plate-type reaction tower 2 from a communicating pipe 4 arranged at the top of the heating kettle 3, the outer wall of the upper part of the plate-type reaction tower 2 is provided with a hexamethyldisiloxane inlet pipe 5, the hexamethyldisiloxane enters the plate-type reaction tower 2 from the hexamethyldisiloxane inlet pipe 5, the heated and dry hydrogen chloride gas introduced from the bottom of the plate-type reaction tower 2 is matched to carry out contact reaction in the plate-type reaction tower 2, and the reacted gaseous trimethyl chlorosilane and chlorine hydride gas rise and then enter the packing rectifying, packing rectifying column 1 top is connected with condenser 8 through outlet duct 7, off-the-shelf trimethylchlorosilane is derived from discharging pipe 10 that sets up on condenser 8 lateral wall, 2 bottoms in plate-type reaction tower are provided with outlet pipe 21, outlet pipe 21 is kept away from one side lateral wall of into hydrogen chloride gas pipe 6 with heating cauldron 3 and is connected, a water that is used for deriving the reaction and obtains, water mixing portion's hydrogen chloride gas forms behind the dilute hydrochloric acid, discharge the processing from the drain pipe 22 of heating cauldron 3 bottoms is unified, through adopting above-mentioned technical scheme, the area of manufacturing cost and equipment has been reduced, moreover, the steam generator is simple in structure, it has improved the transmission efficiency of reactant and resultant to be the structure of folding tower type from top to bottom, and then whole production efficiency has been improved.
In the specific embodiment of the invention, a cooling tank 11 is sleeved outside the condenser 8, a circulating water inlet pipe 12 for introducing cooling water is connected to the side wall of one side of the cooling tank 11, and a circulating water return pipe 13 for leading out the cooling water after heat exchange is connected to the side wall of one side of the cooling tank 11, which is far away from the circulating water inlet pipe 12.
Through adopting above-mentioned technical scheme, establish cooler bin 11 at 8 outside covers of condenser, be connected with circulating water inlet tube 12 on the lateral wall of 11 one sides of cooler bin, be connected with circulating water wet return 13 on the lateral wall of one side that cooler bin 11 kept away from circulating water inlet tube 12, the cooling water enters into cooler bin 11 from circulating water inlet tube 12, and carry out abundant heat transfer with 8 outer walls of condenser, the condensation effect of condenser 8 has further been improved, thereby trimethylchlorosilane's precipitation efficiency has been improved, whole production speed has been improved, the cooling water after the completion heat transfer is derived from circulating water wet return 13.
In the specific embodiment of the invention, the top of the condenser 8 is connected with a gas return pipe 14 for guiding out residual hydrogen chloride gas, one end of the gas return pipe 14, which is far away from the condenser 8, penetrates through the side wall of the cooling tank 11 and then is communicated with the hydrogen chloride gas inlet pipe 6, and a fan 15 is arranged on the gas return pipe 13.
By adopting the technical scheme, in order to further reduce the discharge of the three industrial wastes and simultaneously reduce the production cost and improve the utilization rate of resources, the top of the condenser 8 is connected with a gas return pipe 14 for leading out residual hydrogen chloride gas, one end of the gas return pipe 14, which is far away from the condenser 8, penetrates through the side wall of the cooling box 11 and then is communicated with the hydrogen chloride gas inlet pipe 6, a fan 15 is arranged on the gas return pipe 13, after the fan 15 operates, the negative pressure in the air return pipe 13 is maintained, the residual hydrogen chloride gas is continuously extracted, the hydrogen chloride gas is extracted from the top of the condenser 8 and returned to the hydrogen chloride gas inlet pipe 6, the dry hydrogen chloride gas which is introduced is matched to return to the heating kettle 3 again for heating so as to facilitate the subsequent reaction, the discharge of three wastes is reduced by the cyclic utilization, meanwhile, the introduction amount of hydrogen chloride gas is reduced, the utilization rate of resources is improved, and the production cost and energy consumption are reduced.
In the present embodiment, the hydrogen chloride gas inlet pipe 6 is provided with a hydrogen chloride vent valve 16.
By adopting the technical scheme, in order to conveniently control the introduction amount of the dry hydrogen chloride gas, the dry hydrogen chloride gas is reacted by matching with the input amount of hexamethyldisiloxane so as to promote the balance of the reactants of the reaction, and the hydrogen chloride gas inlet pipe 6 is provided with the hydrogen chloride vent valve 16.
In a specific embodiment of the invention, the plate-type reaction tower 2 comprises a tower body 100 in a vertical cylindrical shape, one end of the communicating pipe 4 far away from the heating kettle 3 is connected with the side wall of the lower part of the tower body 100, a first spray component and a second spray component are respectively arranged in the tower body 100 and above the communicating pipe 4, the first spray component comprises a first annular pipe 111 and a first filter plate 112 which are sequentially arranged from top to bottom, a plurality of first spray pipes 113 are arranged on the side wall of the first annular pipe 111 along the circumferential direction at intervals, the second spray component comprises a second annular pipe 121 and a second filter plate 122 which are sequentially arranged from top to bottom, a plurality of second spray pipes 123 are arranged on the side wall of the second annular pipe 121 along the circumferential direction at intervals, a plurality of retaining ring components for retaining hexamethyldisiloxane gas to cooperate with hydrogen chloride gas to react are uniformly stacked on the upper surfaces of the first filter plate 112 and the second filter plate 122, hexamethyldisiloxane advances 5 one end and is connected with first ring pipe 111 and second ring pipe 121 respectively, hexamethyldisiloxane advances that 5 one ends of keeping away from tower body 100 of pipe are connected with storage hexamethyldisiloxane case 104, hexamethyldisiloxane advances to be provided with on the pipe 5 and sprays pump 105, the tower body bottom is provided with cistern 102, cistern 102 passes through outlet pipe 21 and is connected with 3 lateral walls of heating cauldron, the top of tower body 100 is passed through gas outlet 103 and is linked together with filler rectifying column 1 bottom.
By adopting the technical scheme, the communicating pipe 4 is connected on the side wall of the lower part of the spray tower body 100, the heated and dried hydrogen chloride gas enters the spray tower body 100 from the communicating pipe 4, the hexamethyldisiloxane storage box 104 is arranged on one side of the spray tower body 100, the spray pump 105 is arranged above the hexamethyldisiloxane storage box 104, under the pumping action of the spray pump 105, the raw material hexamethyldisiloxane in the hexamethyldisiloxane storage box 104 is continuously pumped through the hexamethyldisiloxane inlet pipe 5 and is respectively introduced into the first annular pipe 111 and the second annular pipe 121, the plurality of first spray pipes 113 are arranged on the side wall of the first annular pipe 111 at intervals along the circumferential direction, the plurality of second spray pipes 123 are arranged on the side wall of the second annular pipe 121 at intervals along the circumferential direction, and the raw material hexamethyldisiloxane is respectively and uniformly sprayed to the retention filter plate 112 positioned on the upper surface of the first filter plate 122 through the plurality of first spray pipes 113 and the plurality of second spray pipes 123 On the ring subassembly, the retention ring subassembly is evenly piled up the setting at first filter plate 112 and second filter plate 122 upper surface, abundant stay the retention ring subassembly with raw materials hexamethyldisiloxane on, the utilization ratio of raw materials is improved, the big promotion of raw materials handling capacity in the unit interval, a hydrogen chloride gas for the cooperation is risen reacts, the contact surface of hydrogen chloride gas and hexamethyldisiloxane has been increased, thereby the effect of spraying raw materials hexamethyldisiloxane has been improved, and simultaneously, the reaction efficiency of hydrogen chloride gas and raw materials hexamethyldisiloxane has been accelerated, hydrogen chloride gas rises and with raw materials hexamethyldisiloxane contact reaction after, the trimethylchlorosilane who obtains rises and derives through gas outlet 103.
In an embodiment of the present invention, the detaining ring assembly includes a plurality of connecting rings 131 longitudinally spaced from each other at equal intervals and having a same central axis, a central column 132 is disposed on the central axis of the plurality of connecting rings 131, a plurality of detaining plates 133 are disposed on the sidewall of the central column 132 along the circumferential direction and between adjacent connecting rings 131, and the adjacent connecting rings 131 are fixedly connected to each other by the plurality of detaining plates 133.
By adopting the technical scheme, after the first spraying assembly and the second spraying assembly spray and continuously spray the raw material hexamethyldisiloxane onto the retaining ring assembly, the raw material hexamethyldisiloxane is fully retained on the connecting rings 131 and the retaining plates 133, the hydrogen chloride gas is uniformly distributed between the connecting rings 131 and the retaining plates 133 which are longitudinally spaced at equal intervals after rising, the gas-liquid distribution is improved by the structure, the surfaces of the connecting rings 131 and the retaining plates 133 are fully utilized, so that the raw material hexamethyldisiloxane and the hydrogen chloride gas are subjected to full and uniform contact reaction, the treatment capacity is improved by more than fifty percent compared with the prior art, the reaction capacity of the raw material in unit time is greatly improved, the spraying efficiency and the spraying effect are improved, and the purity and quality of the finished product trimethylchlorosilane obtained by reaction are improved.
In the embodiment of the present invention, a plurality of blocking plates 133 are disposed along the circumference of the central pillar 132 at equal intervals, and a reinforcing blocking plate 134 is disposed between two adjacent blocking plates 133.
By adopting the technical scheme, the blocking plates 133 are arranged at intervals along the circumferential direction of the central column 132 at equal intervals, so that the raw material hexamethyldisiloxane sprayed onto the blocking plates 133 and the connecting rings 131 is uniformly distributed on the blocking ring assembly and is uniformly and fully reacted with the rising hydrogen chloride gas, and the reaction efficiency and effect are improved. In order to further improve the retention effect on the hexamethyldisiloxane as the raw material, so as to improve the reaction promoting efficiency and improve the utilization rate of the raw material, a reinforced retention plate 134 is arranged between two adjacent retention plates 133, the integral structural strength of the retention plate assembly is improved, and the service life is prolonged.
In an embodiment of the invention, an end of the first plurality of spray pipes 113 remote from the first annular pipe 111 is offset towards a longitudinal central axis of the tower body 100, and an end of the second plurality of spray pipes 123 remote from the second annular pipe 121 is offset towards the longitudinal central axis of the tower body 100.
Through adopting above-mentioned technical scheme, in order to further improve first spray assembly and second spray assembly's the effect of spraying, guarantee to spray and target in place, the one end of keeping away from first annular pipe 111 with a plurality of first shower 113 is towards the vertical axis skew of spray tower body 100, and the one end of keeping away from second annular pipe 121 with a plurality of second shower 123 is towards the vertical axis skew of spray tower body 100.
In the embodiment of the present invention, the connecting ring 131, the central column 132, the blocking plate 133 and the reinforced blocking plate 134 are made of glass-lined and fluorine-containing plastic.
By adopting the technical scheme, in order to further prolong the service life of the retention plate assembly and prevent the corrosion of hydrogen chloride gas, the connecting ring 131, the central column 132, the retention plate 133 and the reinforced retention plate 134 are all made of glass lining fluorine-containing plastic.
The invention also discloses a production method of the production line for producing trimethylchlorosilane by the tower stacking method, which has low energy consumption and high cyclic utilization rate, and comprises the following steps:
1) and raw material feeding: the spraying pump 105 operates normally, hexamethyldisiloxane in the hexamethyldisiloxane storage box 104 is pumped and continuously introduced into the first annular pipe 111 and the second annular pipe 121 in the plate-type reaction tower 2 through the hexamethyldisiloxane inlet pipe 5, and is sprayed downwards from a plurality of first spraying pipes 113 arranged on the side wall of the first annular pipe 111 and a plurality of second spraying pipes 123 arranged on the side wall of the second annular pipe 121, and the flow rate of the hexamethyldisiloxane is controlled by the spraying pump 105 to be 200 kg/h;
2) and introducing reactants: opening a hydrogen chloride vent valve 16, introducing the dried hydrogen chloride gas into the heating kettle 3 from a hydrogen chloride gas inlet pipe 6, operating the heating kettle 3 and heating the dried hydrogen chloride gas, introducing the heated hydrogen chloride gas into the plate-type reaction tower 2 from a communicating pipe 4 arranged at the top of the heating kettle 3, and controlling the flow of the dried hydrogen chloride gas to be 110 kg/h;
3) and reaction rectification: hexamethyldisiloxane is respectively and uniformly sprayed to a blocking ring assembly positioned on the upper surfaces of the first filter plate 112 and the second filter plate 122 and is fully blocked on a plurality of connecting rings 131, a central column 132 and a plurality of blocking plates 133, the heated and dried hydrogen chloride gas rises from the bottom of the plate-type reaction tower 2 and reacts with the hexamethyldisiloxane, the gas rises from a gas outlet 103 at the top of the plate-type reaction tower 2 after reaction and enters the packing rectifying tower 1 for rectification, the reacted water mixed with hydrogen chloride forms dilute hydrochloric acid liquid, the dilute hydrochloric acid liquid falls into a water reservoir 102, the dilute hydrochloric acid liquid flows back into the heating kettle 3 from a water outlet pipe 21, and the dilute hydrochloric acid liquid is led out through a liquid outlet pipe 22 arranged at the bottom of the heating kettle 3;
4) condensing and refluxing: the condenser 8 works, cooling water is continuously introduced into the cooling tank 11 from a circulating water inlet pipe 12, the cooling water is cooled by matching with the cooler 8, the cooling water after heat exchange is led out from a circulating water return pipe 13, gaseous hydrogen chloride and trimethylchlorosilane rise and enter the condenser 8 from an air outlet pipe 7, a trimethylchlorosilane finished product is led out from a discharge pipe 10 on the side wall of the condenser 8 under the condensation effect, and part of liquid flows back to the packing rectifying tower 1 from the bottom of the condenser 8 through a return pipe 9 to be rectified again to improve the purity;
5) and (3) circulating reaction: and (3) opening the fan 15 to maintain the micro negative pressure in the air return pipe 14 to be 0-0.01 Mpa, pumping the residual hydrogen chloride gas in the condenser 8 from the air return pipe 14 back to the hydrogen chloride gas inlet pipe 6, and returning the residual hydrogen chloride gas to the heating kettle 3 to be mixed with the dry hydrogen chloride gas for reheating and recycling.
By adopting the technical scheme, trimethylchlorosilane is produced by utilizing a tower-stacking method, a packing rectifying tower 1, a plate type reaction tower 2 and a heating kettle 3 for reaction are sequentially arranged from top to bottom, so that various conveying devices for conveying reactants and products are reduced, the production line is simplified, the production cost is reduced, the floor area of the production device is reduced, the structure is relatively simple, on the other hand, dry hydrogen chloride gas quickly rises into the plate type reaction tower 2 after entering the heating kettle 3 for heating, the dry hydrogen chloride gas is in full contact reaction with hexamethyldisiloxane in the plate type reaction tower 2, the reaction efficiency is improved, meanwhile, the hexamethyldisiloxane is fully retained by a retaining ring assembly arranged in the plate type reaction tower 2, the spraying effect of a first spraying assembly and a second spraying assembly is matched, and the dry and heated hydrogen chloride gas which rises from bottom to top is subjected to uniform contact reaction, the overall efficiency of the reaction is improved, the residual hydrogen chloride gas in the condenser 8 after the reaction is finished is pumped back into the hydrogen chloride gas inlet pipe 6 from the gas return pipe 14, and flows back to the heating kettle 3 to be heated again for recycling after being mixed with the dry hydrogen chloride gas, thereby improving the overall resource recycling rate, thereby further reducing the overall production cost and reducing the emission of waste gas, further improving the precipitation efficiency of the trimethylchlorosilane product by matching the cooling tank 11 with the condenser 8, improving the overall production speed, and simultaneously, the invention provides a production line and a production method for producing trimethylchlorosilane by a tower-stacking method, wherein the production line has the advantages of low production cost, simple structure, high production efficiency, good reaction promoting effect, high recovery rate and long service life.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (10)
1. A production line for producing trimethylchlorosilane by a tower stacking method is characterized in that: comprises a packing rectifying tower (1), a plate-type reaction tower (2) and a heating kettle (3) which are sequentially arranged from top to bottom, wherein the bottom of the packing rectifying tower (1) is communicated with the top of the plate-type reaction tower (2), the top of the heating kettle (3) is connected with the lower side wall of the plate-type reaction tower (2) through a communicating pipe (4), a hexamethyldisiloxane inlet pipe (5) is arranged on the outer wall of the upper part of the plate-type reaction tower (2), a hydrogen chloride inlet gas pipe (6) for leading in dry hydrogen chloride gas is connected onto the side wall of the heating kettle (3), a condenser (8) is connected onto the top of the packing rectifying tower (1) through an outlet pipe (7), the bottom of the condenser (8) is connected with the upper side wall of the packing rectifying tower (1) through a return pipe (9), and a chlorosilane discharging pipe (10) for leading out trimethyl is arranged on, plate-type reaction tower (2) bottom is kept away from into one side lateral wall of hydrogen chloride gas pipe (6) through outlet pipe (21) and heating cauldron (3) and is connected, heating cauldron (3) bottom is provided with drain pipe (22) that are used for deriving the dilute hydrochloric acid.
2. The production line of trimethylchlorosilane by the stacked tower method as claimed in claim 1, is characterized in that: condenser (8) outside cover is equipped with cooler bin (11), be connected with circulating water inlet tube (12) that are used for letting in the cooling water on the lateral wall of cooler bin (11) one side, be connected with circulating water wet return (13) that are used for deriving the cooling water after the heat transfer on the lateral wall of one side that circulating water inlet tube (12) was kept away from in cooler bin (11).
3. The production line of trimethylchlorosilane by the stacked tower method as claimed in claim 2, is characterized in that: condenser (8) top is connected with muffler (14) that are used for deriving surplus hydrogen chloride gas, muffler (14) are kept away from behind condenser (8) the one end run through cooling tank (11) lateral wall with advance hydrogen chloride gas pipe (6) intercommunication, be provided with fan (15) on muffler (13).
4. The production line of trimethylchlorosilane by the stacked tower method as claimed in claim 3, is characterized in that: and a hydrogen chloride vent valve (16) is arranged on the hydrogen chloride inlet gas pipe (6).
5. A production line for producing trimethylchlorosilane by a stack process according to claim 1, 2 or 3, characterized in that: plate-type reaction tower (2) is including being vertical cylindric tower body (100), the one end and tower body (100) lower part lateral wall that heating cauldron (3) were kept away from to communicating pipe (4) are connected, tower body (100) are inside and lie in communicating pipe (4) top and be provided with first spray assembly and second spray assembly respectively, first spray assembly includes from last first ring pipe (111) and first filter plate (112) down set gradually, be provided with a plurality of first shower (113) along circumference equidistance interval each other on first ring pipe (111) lateral wall, the second spray assembly includes from last second ring pipe (121) and the second filter plate (122) that down set gradually, be provided with a plurality of second shower (123) along circumference equidistance interval each other on second ring pipe (121) lateral wall, first filter plate (112) and second filter plate (122) upper surface all evenly pile up and are provided with a plurality of being used for hindering and stay hexamethyldisiloxane cooperation hydrogen chloride gas The body carries out the trapping ring subassembly that reacts, hexamethyldisiloxane advances pipe (5) one end and is connected with first ring pipe (111) and second ring pipe (121) respectively, hexamethyldisiloxane advances one end that pipe (5) kept away from tower body (100) and is connected with storage hexamethyldisiloxane case (104), hexamethyldisiloxane advances to be provided with on pipe (5) and sprays pump (105), the tower body bottom is provided with cistern (102), cistern (102) are connected with heating cauldron (3) lateral wall through outlet pipe (21), gas outlet (103) and filler rectifying column (1) bottom intercommunication are passed through to tower body (100) top.
6. The production line of trimethylchlorosilane by the stacked tower method as claimed in claim 5, is characterized in that: the detaining ring assembly comprises a plurality of connecting rings (131) which are distributed on the same central shaft at equal intervals along the longitudinal direction, a central column (132) is arranged on the central shaft of the connecting rings (131), a plurality of detaining plates (133) are arranged on the side wall of the central column (132) along the circumferential direction and between the adjacent connecting rings (131), and the adjacent connecting rings (131) are fixedly connected with each other through the plurality of detaining plates (133).
7. The production line of trimethylchlorosilane by the stacked tower method as claimed in claim 6, is characterized in that: the blocking plates (133) are arranged at intervals along the circumferential direction of the central column (132) at equal intervals, and a reinforcing blocking plate (134) is arranged between every two adjacent blocking plates (133).
8. The production line of trimethylchlorosilane by the stacked tower method as claimed in claim 5, is characterized in that: one end of the first spray pipes (113) far away from the first annular pipe (111) is deviated towards the longitudinal central axis of the tower body (100), and one end of the second spray pipes (123) far away from the second annular pipe (121) is deviated towards the longitudinal central axis of the tower body (100).
9. The production line of trimethylchlorosilane by the stacked tower method as claimed in claim 7, is characterized in that: the connecting ring (131), the central column (132), the blocking plate (133) and the reinforced blocking plate (134) are all made of glass lining and fluorine-containing plastic.
10. A method for producing trimethylchlorosilane using the production line according to any one of claims 6 to 7 and 9, comprising the steps of:
1) and raw material feeding: the spraying pump (105) runs normally, hexamethyldisiloxane in the hexamethyldisiloxane storage box (104) is pumped and continuously introduced into a first annular pipe (111) and a second annular pipe (121) in the plate-type reaction tower (2) through the hexamethyldisiloxane inlet pipe (5), and the hexamethyldisiloxane is sprayed downwards from a plurality of first spraying pipes (113) arranged on the side wall of the first annular pipe (111) and a plurality of second spraying pipes (123) arranged on the side wall of the second annular pipe (121), and the flow rate of the hexamethyldisiloxane is controlled by the spraying pump (105) to be 200 kg/h;
2) and introducing reactants: opening a hydrogen chloride vent valve (16), introducing dry hydrogen chloride gas into a heating kettle (3) from a hydrogen chloride gas inlet pipe (6), operating the heating kettle (3) and heating the dry hydrogen chloride gas, introducing the heated hydrogen chloride gas into a plate-type reaction tower (2) from a communicating pipe (4) arranged at the top of the heating kettle (3), and controlling the flow of the dry hydrogen chloride gas to be 110 kg/h;
3) and reaction rectification: hexamethyldisiloxane is respectively and uniformly sprayed to a blocking ring assembly on the upper surfaces of a first filter plate 112 and a second filter plate 122 and is fully blocked on a plurality of connecting rings (131), a central column (132) and a plurality of blocking plates (133), hydrogen chloride gas heated and dried rises from the bottom of a plate-type reaction tower (2) and reacts with the hexamethyldisiloxane, the gas rises from a gas outlet (103) at the top of the plate-type reaction tower (2) after reaction and enters a packing rectifying tower (1) for rectification, the reacted water is mixed with hydrogen chloride to form dilute hydrochloric acid liquid, the dilute hydrochloric acid liquid falls into a reservoir (102), the dilute hydrochloric acid liquid flows back into a heating kettle (3) from a water outlet pipe (21), and the dilute hydrochloric acid liquid is led out through a liquid outlet pipe (22) arranged at the bottom of the heating kettle (3);
4) condensing and refluxing: the condenser (8) works, cooling water is continuously introduced into the condenser (8) and enters the cooling box (11) from the circulating water inlet pipe (12) to be matched with the cooler (8) for cooling, the cooling water after heat exchange is led out from the circulating water return pipe (13), gaseous hydrogen chloride and trimethylchlorosilane rise and enter the condenser (8) from the gas outlet pipe (7), a trimethylchlorosilane finished product is led out from the discharge pipe (10) on the side wall of the condenser (8) under the condensation effect, and partial liquid flows back to the filler rectifying tower (1) from the bottom of the condenser (8) through the return pipe (9) to be rectified again to improve the purity;
5) and (3) circulating reaction: and (3) opening the fan (15), keeping the micro negative pressure in the air return pipe (14) between 0 and-0.01 Mpa, pumping the residual hydrogen chloride gas in the condenser (8) from the air return pipe (14) back to the hydrogen chloride gas inlet pipe (6), and returning the residual hydrogen chloride gas to the heating kettle (3) to be mixed with the dry hydrogen chloride gas for reheating and recycling.
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| CN105367594A (en) * | 2015-10-09 | 2016-03-02 | 浙江硕而博化工有限公司 | Method for preparing hexamethyl-disilazane with hexamethyldisiloxane as raw material |
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| CN105367594A (en) * | 2015-10-09 | 2016-03-02 | 浙江硕而博化工有限公司 | Method for preparing hexamethyl-disilazane with hexamethyldisiloxane as raw material |
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| 三甲基氯硅烷及其下游产物的合成研究;夏易君;《中国优秀硕士论文全文数据库》;20080415;第2-3节 * |
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